CN105541628A - Method for recycling dioctyl phthalate - Google Patents
Method for recycling dioctyl phthalate Download PDFInfo
- Publication number
- CN105541628A CN105541628A CN201610023975.5A CN201610023975A CN105541628A CN 105541628 A CN105541628 A CN 105541628A CN 201610023975 A CN201610023975 A CN 201610023975A CN 105541628 A CN105541628 A CN 105541628A
- Authority
- CN
- China
- Prior art keywords
- reaction
- diop
- virahol
- stirring
- dioctyl phthalate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/56—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
Abstract
The invention relates to a method for recycling dioctyl phthalate, and belongs to the technical field of organic compounds. The method includes the steps that filter residues generated in the industrial production process serve as raw materials, alcohol serves as an extraction solvent, heating and stirring are carried out with the stirring speed decreased gradually to conduct an active carbon desorption reaction, reaction liquid is obtained through suction filtration after the desorption reaction is finished, and a filter cake is rinsed two times; the reaction liquid is subjected to reduced-pressure distillation to obtain the product DIOP and the solvent isopropanol, and the solvent is recycled to be reused. The method is applied to recycling and reusing of DIOP in waste filter residues, DIOP production cost can be reduced, cleanliness and environmental friendliness can be achieved, and beneficial reusing of waste can be achieved.
Description
Technical field
The present invention relates to a kind of recovery method of dioctyl phthalate (DOP), belong to organic compound technical field.
Background technology
Phthalate (1C ~ 13C) has another name called titanic acid ester (PAEs), is current domestic application softening agent widely, accounts for 80% of whole softening agent output.It has excellent processing characteristics, cost is low, plasticizing efficiency is high, be applied to can reduce plastic prod in polyethylene and polyvinyl chloride material modulus, hardness, embrittlement and softening temperature, can also increase product snappiness, plasticity-and draw high performance, it is also widely used in the fields such as coating, agricultural chemicals, dyestuff, ink, lubricating oil, washing composition and tensio-active agent.In the U.S., Canada, European Union and China, the phthalate of low carbon chain (3C ~ 6C) is replaced by high carbon chain (>6C) gradually, their volatility and transport property little, resistance to extraction performance is good.Along with the growth gradually of carbochain, its compatible stability as additive is also more and more stronger.Dioctyl phthalate (DOP) (DIOP) is a kind of primary plasticizer of better performances, has a wide range of applications.
The structural formula of dioctyl phthalate (DOP) (DIOP) is as follows:
In the actual production process of DIOP, reacted product does not often reach requirement in colourity, often needs with a large amount of activated carbon decolorizings.Containing about 1.5% octanol, about 0.8% phthalic anhydride of the DIOP and minute quantity that account for total mass ratio 60 ~ 65% in gac filter residue after decolouring.This part gac filter residue is burnt by as refuse derived fuel, so not only wasted raw material but also contaminate environment, the present invention's alcohols material is recycled the waste the DIOP in filter residue, especially unexpected technique effect is obtained with Virahol as extraction agent, and determine optimum experimental condition, the DIOP of content more than 90% can be reclaimed, again reduce the organic content of 47% of filter residue absorption.Clean environment firendly and can realize changing waste into resources utilize, production cost can be reduced and alleviate environmental pollution, from waste filter residue, reclaiming DIOP about this type of and then rarely have similar report.
Based on this, make the application.
Summary of the invention
In order to overcome the above-mentioned problems in the prior art, the invention provides one can high efficiente callback DIOP, realizes the recovery method of the dioctyl phthalate (DOP) that changing waste into resources utilizes.
For achieving the above object, the technical scheme taked of the present invention is as follows:
A recovery method for dioctyl phthalate (DOP), comprises the steps:
(1) be raw material with the filter residue produced in Industrial processes, using alcohol as Extraction solvent, heated and stirred carries out gac desorption reaction, and first quick and back slow, after desorption reaction, suction filtration goes out reaction solution to stirring velocity, and twice rinse filter cake;
(2) reaction solution underpressure distillation obtains product D IOP and solvent Virahol, and solvent recuperation is for recycle.
Further, as preferably:
In step (1), the mass ratio of filter residue and alcohol is 1:(0.5 ~ 3), desorption reaction temperature is 30 ~ 100 DEG C, and the reaction times is 0.5 ~ 3 hour.More preferred, described filter residue and the mass ratio of alcohol are 1:(1 ~ 2), desorption reaction temperature is 45 ~ 70 DEG C, and the reaction times is 0.75 ~ 1.5 hour.
In step (1), stirring is divided into pre-stirring and reaction stirring, and advanced line speed at the pre-stirring 5-20 minute of 80-120r/min, then carries out reaction stirring 40-60 minute under 250-400r/min speed.More preferred, described pre-stirring velocity is 100r/min, and the time is 8-12 minute; Reaction stirring velocity is 300r/min, and the time is 45-55 minute.
In step (1), described Extraction solvent can select the one in the alcohols such as methyl alcohol, ethanol, propyl alcohol, Virahol, butanols, amylalcohol.
In step (2), described vacuum distillation temperature is 70 ~ 80 DEG C, and pressure is-0.1 ~-0.3MPa.More preferred, described vacuum distillation temperature is 78 DEG C, and pressure is-0.1 ~-0.15MPa.
Principle of work of the present invention and beneficial effect as follows:
(1) the present invention adopts alcohols as specific extraction agent, this type of extraction agent and DIOP mutual solubility good, and be easily separated with DIOP, substantially pollution-free to environment, disposablely under appropriate conditions from waste filter residue, extract the DIOP accounting for total content 90%, higher by 20 ~ 25% as the extraction efficiency of solvent than 95% ethanol, and extraction agent is capable of circulation reuses, the product DIOP extracted uses as thick finished product, DIOP production cost can be reduced, clean environment firendly and realize changing waste into resources utilize, when especially adopting Virahol as extraction agent, under same experimental conditions, 22% is improved as extraction agent than with the ester yield of extraction using alcohol agent with Virahol, and solvent recovering rate reduces by 3.6 ~ 4.8%, for the reduction by 14 ~ 15% by the organic content ratio Ethanol Treatment of adsorbing in the filter residue after Virahol process.
(2) with the filter residue after Virahol process than the content few 15 ~ 16% with the filter residue adsorb organic compound after 95% Ethanol Treatment, than the content few 46.2 ~ 49.2% of untreated filter residue adsorb organic compound, greatly reduce with the content of filter residue adsorb organic compound after Virahol process, the pollution of environment is greatly weakened; Simultaneously, by the control to processing condition in removal process, as the proportioning between different substances, temperature of reaction and the setting in reaction times, optimum balance effect can be realized: disposable ester yield is 89.1%, solvent recovering rate is 66.5%, and before and after filter residue process, the content difference of adsorb organic compound is 46.3%.
The DIOP that the present invention's alcohols is recycled the waste in filter residue as Virahol etc., disposable from filter residue extraction account for the DIOP of total content 90%, higher by 20 ~ 25% as the extraction efficiency of solvent than 95% ethanol, after making process the organic content of filter residue greatly reduce (account for the DIOP of total mass ratio 6 ~ 8%, about 0.5% octanol, the phthalic anhydride of about 0.5% and the Virahol of 8 ~ 9%)
Clean environment firendly and can realize changing waste into resources utilize, production cost can be reduced and alleviate environmental pollution.
Accompanying drawing explanation
Fig. 1 is the trend map of temperature to ester yield, solvent recovering rate;
Fig. 2 is the trend map of proportioning to ester yield, solvent recovering rate;
Fig. 3 is the trend map of time to ester yield, solvent recovering rate
Embodiment
Embodiment 1 and 2 using 95% ethanol as Extraction solvent, and compares, specifically see embodiment 1, embodiment 2 and table 1 residual organic content after extraction DIOP effect, solvent recovering rate and process filter residue.
Embodiment 1
1) in 500mL four-hole boiling flask, filter residue 150g is added, ethanol 150g, temperature of reaction is 50 DEG C, just having started stirring velocity is 100r/min, stir 10min, after to tune up stirring velocity be 300r/min, continue to stir 80min, reacted material is carried out suction filtration 1h while hot, obtains black filter cake and light yellow filtrate.
2) get ethanol 50g, (25g) repeated washing filter cake, drains filter cake in two batches.
3), at temperature 70 C, under pressure-0.10MPa, underpressure distillation filtrate, obtains product DIOP, and recycling design ethanol recycled in order to next time.
Embodiment 2
1) in 500mL four-hole boiling flask, filter residue 150g is added, ethanol 300g, temperature of reaction is 50 DEG C, just having started stirring velocity is 100r/min, stir 10min, after to tune up stirring velocity be 300r/min, continue to stir 80min, reacted material is carried out suction filtration 1h while hot, obtains black filter cake and light yellow filtrate.
2) get ethanol 50g, (25g) repeated washing filter cake, drains filter cake in two batches.
3), at temperature 70 C, under pressure-0.10MPa, underpressure distillation filtrate, obtains product DIOP, and recycling design ethanol recycled in order to next time.
Table 1 ethanol is as the extraction effect synopsis of Extraction solvent
In table 1, organic content difference refers to the content difference of adsorb organic compound before and after filter residue process.
Ester yield is that the mass ratio by reclaiming total DIOP content in DIOP and filter residue obtains, and reclaims DIOP: total DIOP=67.7 ~ 68.2%; Solvent recovering rate is obtained by the mass ratio of recycling design and total solvent, recycling design: total solvent=65.3 ~ 68.3%.
The DIOP adsorbed in filter residue, isooctyl alcohol, phthalic anhydride and amount of alcohol are mutually verified by liquid phase chromatography and thermogravimetry to obtain, and in table 1, the experimental data of ester yield has also confirmed the accuracy of the DIOP content difference of filter residue absorption before and after process.
Process before filter residue absorption organic content (account for the DIOP of total mass ratio 60 ~ 61%, about 1.5% isooctyl alcohol and 0.8% phthalic anhydride); With the organic content of filter residue absorption after Ethanol Treatment (account for the DIOP of total mass ratio 20 ~ 21%, about 0.5% isooctyl alcohol, the phthalic anhydride of about 0.5% and the ethanol of 10 ~ 11%).
Embodiment 3 and 4 using Virahol as extraction agent, and compares, specifically see embodiment 3, embodiment 4 and table 2 residual organic content after extraction DIOP effect, solvent recovering rate and process filter residue.
Embodiment 3
1) in 500mL four-hole boiling flask, filter residue 150g is added, Virahol 150g, temperature of reaction is 50 DEG C, just having started stirring velocity is 100r/min, stir 10min, after to tune up stirring velocity be 300r/min, continue to stir 80min, reacted material is carried out suction filtration 1h while hot, obtains black filter cake and light yellow filtrate.
2) get Virahol 50g, (25g) repeated washing filter cake, drains filter cake in two batches.
3), temperature 78 DEG C, under pressure-0.10MPa, underpressure distillation filtrate, obtains product DIOP, and recycling design Virahol recycled in order to next time.
Embodiment 4
1) in 500mL four-hole boiling flask, filter residue 150g is added, Virahol 300g, temperature of reaction is 50 DEG C, just having started stirring velocity is 100r/min, stir 10min, after to tune up stirring velocity be 300r/min, continue to stir 80min, reacted material is carried out suction filtration 1h while hot, obtains black filter cake and light yellow filtrate.
2) get Virahol 50g, (25g) repeated washing filter cake, drains filter cake in two batches.
3), temperature 78 DEG C, under pressure-0.10MPa, underpressure distillation filtrate, obtains product DIOP, and recycling design Virahol recycled in order to next time.
Table 2 Virahol is as the extraction effect synopsis of Extraction solvent
The rate of recovery of DIOP and solvent Virahol, in table 2 results of comparison, reclaims DIOP: total DIOP=89.7 ~ 90.7%; Recycling design: total solvent=60.3 ~ 64.7%.
Process before filter residue absorption organic content: account for the DIOP of total mass ratio 60 ~ 61%, about 1.5% isooctyl alcohol and 0.8% phthalic anhydride; Organic content with filter residue absorption after Virahol process: account for the DIOP of total mass ratio 6 ~ 7%, about 0.5% isooctyl alcohol, the phthalic anhydride of about 0.5% and the Virahol of 8 ~ 9%.
Data Comparison through table 1 and table 2 can be found out, 22% is improve as the ester yield of extraction agent ratio extraction using alcohol agent with Virahol, and solvent recovering rate reduces 3.6 ~ 4.8%, for the reduction by 14 ~ 15% by the organic content ratio Ethanol Treatment of adsorbing in the filter residue after Virahol process, consider ester yield, the impact that in solvent recovering rate and filter residue, organic content causes environment, adopt Virahol as extraction agent, it extracts DIOP effect, solvent recovering rate and the organic content remained after processing filter residue are all better than ethanol as extraction agent, achieve unexpected effect.
Embodiment 5-9, using Virahol as extraction agent, has investigated proportioning, temperature and reaction times respectively on ester yield, solvent recovering rate and the impact on organic amount contained by filter residue.
Embodiment 5
1) in 500mL four-hole boiling flask, filter residue 150g is added, Virahol 150g, temperature of reaction is 30 DEG C, just having started stirring velocity is 100r/min, stir 10min, after to tune up stirring velocity be 300r/min, continue to stir 80min, reacted material is carried out suction filtration 1h while hot, obtains black filter cake and light yellow filtrate.
2) get Virahol 50g, (25g) repeated washing filter cake, drains filter in two batches.
3), temperature 78 DEG C, under pressure-0.10MPa, underpressure distillation filtrate, obtains product DIOP, and recycling design Virahol recycled in order to next time.
Embodiment 6
1) in 500mL four-hole boiling flask, filter residue 150g is added, Virahol 150g, temperature of reaction is 70 DEG C, just having started stirring velocity is 100r/min, stir 10min, after to tune up stirring velocity be 300r/min, continue to stir 80min, reacted material is carried out suction filtration 1h while hot, obtains black filter cake and light yellow filtrate.
2) get Virahol 50g, (25g) repeated washing filter cake, drains filter cake in two batches.
3), temperature 78 DEG C, under pressure-0.10MPa, underpressure distillation filtrate, obtains product DIOP, and recycling design Virahol recycled in order to next time.
Embodiment 7
1) in 500mL four-hole boiling flask, filter residue 150g is added, Virahol 450g, temperature of reaction is 50 DEG C, just having started stirring velocity is 100r/min, stir 10min, after to tune up stirring velocity be 300r/min, continue to stir 80min, reacted material is carried out suction filtration 1h while hot, obtains black filter cake and light yellow filtrate.
2) get Virahol 50g, (25g) repeated washing filter cake, drains filter cake in two batches.
3), temperature 78 DEG C, under pressure-0.10MPa, underpressure distillation filtrate, obtains product DIOP, and recycling design Virahol recycled in order to next time.
Embodiment 8
1) in 500mL four-hole boiling flask, filter residue 150g is added, Virahol 150g, temperature of reaction is 50 DEG C, just having started stirring velocity is 100r/min, stir 10min, after to tune up stirring velocity be 300r/min, continue to stir 20min, reacted material is carried out suction filtration 1h while hot, obtains black filter cake and light yellow filtrate.
2) get Virahol 50g, (25g) repeated washing filter cake, drains filter cake in two batches.
3), temperature 78 DEG C, under pressure-0.10MPa, underpressure distillation filtrate, obtains product DIOP, and recycling design Virahol recycled in order to next time.
Embodiment 9
1) in 500mL four-hole boiling flask, filter residue 150g is added, Virahol 150g, temperature of reaction is 50 DEG C, just having started stirring velocity is 100r/min, stir 10min, after to tune up stirring velocity be 300r/min, continue to stir 50min, reacted material is carried out suction filtration 1h while hot, obtains black filter cake and light yellow filtrate.
2) get Virahol 50g, (25g) repeated washing filter cake, drains filter cake in two batches.
3), temperature 78 DEG C, under pressure-0.10MPa, underpressure distillation filtrate, obtains product DIOP, and recycling design Virahol recycled in order to next time.
Table 3 Virahol is as the extraction effect synopsis of Extraction solvent
Table 3 associative list 2 can be found out, before and after ester yield and filter residue process, the content difference of adsorb organic compound is negative correlation, and namely ester yield raises, and before and after filter residue process, the content difference of adsorb organic compound is corresponding in a certain proportion of reduction, and vice versa.
Embodiment 10-12 is the impact of desorption conditions on the rate of recovery.
Embodiment 10
1) in 500mL four-hole boiling flask, filter residue 150g is added, Virahol 100g, temperature of reaction is 45 DEG C, just having started stirring velocity is 100r/min, stir 10min, after to tune up stirring velocity be 300r/min, continue to stir 50min, reacted material is carried out suction filtration 1h while hot, obtains black filter cake and light yellow filtrate.
2) get Virahol 50g, (25g) repeated washing filter cake, drains filter cake in two batches.
3), temperature 78 DEG C, under pressure-0.10MPa, underpressure distillation filtrate, obtains product DIOP, and recycling design Virahol recycled in order to next time.
Embodiment 11
1) in 500mL four-hole boiling flask, filter residue 150g is added, Virahol 150g, temperature of reaction is 50 DEG C, just having started stirring velocity is 100r/min, stir 10min, after to tune up stirring velocity be 300r/min, continue to stir 80min, reacted material is carried out suction filtration 1h while hot, obtains black filter cake and light yellow filtrate.
2) get Virahol 50g, (25g) repeated washing filter cake, drains filter cake in two batches.
3), temperature 78 DEG C, under pressure-0.10MPa, underpressure distillation filtrate, obtains product DIOP, and recycling design Virahol recycled in order to next time.
Embodiment 12
1) in 500mL four-hole boiling flask, filter residue 150g is added, Virahol 225g, temperature of reaction is 50 DEG C, just having started stirring velocity is 100r/min, stir 10min, after to tune up stirring velocity be 300r/min, continue to stir 35min, reacted material is carried out suction filtration 1h while hot, obtains black filter cake and light yellow filtrate.
2) get Virahol 50g, (25g) repeated washing filter cake, drains filter cake in two batches.
3), temperature 78 DEG C, under pressure-0.10MPa, underpressure distillation filtrate, obtains product DIOP, and recycling design Virahol recycled in order to next time.
Table 4 is the DIOP of embodiment 10-12 and the rate of recovery synopsis of solvent Virahol
Table 4DIOP and isopropanol recovering rate synopsis
The rate of recovery of DIOP and solvent Virahol is in table 4 experimental data, wherein ester yield is obtained by the mass ratio of DIOP content total in recovery DIOP and filter residue, reclaim DIOP: total DIOP=85.4 ~ 90.7%, solvent recovering rate is obtained by the mass ratio of recycling design and total solvent, recycling design: total solvent=64.1 ~ 70.7%.
The DIOP adsorbed in filter residue, octanol, phthalic anhydride and Virahol amount mutually verified by liquid phase chromatography and thermogravimetry to obtain, and in table 4, the experimental data of mass ratio has also confirmed the accuracy of the DIOP content difference of filter residue absorption before and after process: the organic content of filter residue absorption before process (account for the DIOP of total mass ratio 60 ~ 65%, about 1.5% octanol and 0.8% phthalic anhydride); With the organic content of filter residue absorption after Virahol process (account for the DIOP of total mass ratio 6 ~ 8%, about 0.5% octanol, the phthalic anhydride of about 0.5% and the Virahol of 8 ~ 9%).
Embodiment 13-19: desorption temperature is on the impact of the rate of recovery
The operation sequence of this group embodiment is mainly as follows:
1) mass ratio controlling filter residue and Virahol is 1:2, filter residue and Virahol is added in 500mL four-hole boiling flask, and control temperature of reaction, just having started stirring velocity is 100r/min, stir 10min, after to tune up stirring velocity be 300r/min, continue to stir 50min, reacted material is carried out suction filtration 1h while hot, obtains black filter cake and light yellow filtrate.
2) get Virahol, repeated washing filter cake, drains filter cake in two batches.
3), temperature 78 DEG C, under pressure-0.10MPa, underpressure distillation filtrate, obtains product DIOP, and recycling design Virahol recycled in order to next time.
The concrete technology parameter of desorption and rate of recovery ginseng are shown in Table 5.
Table 5DIOP and isopropanol recovering rate synopsis
Along with the rising of temperature, in solvent and filter residue, contained organism activity strengthens gradually, and therefore, the rate of recovery of DIOP can along with the increase gradually of the rising of temperature, and corresponding solvent utilization ratio also can be more and more higher; When temperature exceeds certain limit, solvent there will be a large amount of volatilizations, at high temperature also can there is the side reactions such as pyrolysis in DIOP, thus affect actual recovered rate, therefore, can obviously find out from table 5, only has temperature at 30-90, especially, time in 45-70 DEG C of interval range, solvent activity and filter residue activity are in most matching status, DIOP can well be reclaimed in waste residue.
Embodiment 20-23: underpressure distillation is on the impact of the rate of recovery
Underpressure distillation is mainly for the recovery with solvent that removes of DIOP, and the operation sequence of this group embodiment is mainly as follows:
1) mass ratio controlling filter residue and Virahol is 1:2, filter residue and Virahol is added in 500mL four-hole boiling flask, and to control temperature of reaction be 50 DEG C, just having started stirring velocity is 100r/min, stir 10min, after to tune up stirring velocity be 300r/min, continue to stir 50min, reacted material is carried out suction filtration 1h while hot, obtains black filter cake and light yellow filtrate.
2) get Virahol, repeated washing filter cake, drains filter cake in two batches.
3) control vacuum distillation temperature and pressure, underpressure distillation filtrate, obtains product DIOP, and recycling design Virahol recycled in order to next time.
Wherein, the concrete technology parameter of underpressure distillation and rate of recovery ginseng are shown in Table 6.
Table 6DIOP and isopropanol recovering rate synopsis
Can be found out by table 6, along with the increase of pressure, solvent recovering rate can reduce gradually, and time near-0.1MPa, Virahol can be on best gas-liquid line of balance, is therefore conducive to most the recovery of solvent, and its rate of recovery can reach about 70%.
See proportioning, temperature and the reaction times trend to result in order to clearer, Fig. 1 is the trend map that ester yield (with the content difference of adsorb organic compound before and after filter residue process in negative proportionlity) is formed temperature with solvent recovering rate.As shown in Figure 1, desorption reaction temperature is increased to 50 DEG C by 30 DEG C, and ester yield has obvious lifting, continues to be increased to 70 DEG C, and the change of ester yield is little, and solvent recovering rate raises linearly downtrending with temperature, so temperature of reaction is that 50 DEG C of effects are better.
As shown in Figure 2, along with the lifting of Virahol/filter residue proportioning, ester yield is without considerable change, but solvent recovering rate is on a declining curve, so Virahol/filter residue proportioning is 1:1.
As shown in Figure 3, the reaction times extends to 1h by 0.5h, and ester yield has obvious lifting, and continue time expand to 1.5h, ester yield is without considerable change, and solvent recovering rate raises linearly downtrending with temperature, so the reaction times is that 1h effect is better.
According to proportioning, temperature and reaction times on ester yield, solvent recovering rate and the impact on adsorb organic compound content difference before and after filter residue process, determine best route: Virahol/filter residue proportioning is 1:1, reaction times is 1h, temperature of reaction is 50 DEG C, ester yield is 89.1%, solvent recovering rate is 66.5%, and before and after filter residue process, the content difference of adsorb organic compound is 46.3%.
Above content is the further description done provided technical scheme in conjunction with the preferred implementation of the invention; can not assert that the invention is specifically implemented to be confined to these explanations above-mentioned; for the invention person of an ordinary skill in the technical field; without departing from the concept of the premise of the invention; some simple deduction or replace can also be made, all should be considered as the protection domain belonging to the invention.
Claims (8)
1. a recovery method for dioctyl phthalate (DOP), is characterized in that comprising the steps:
(1) take filter residue as raw material, alcohol is Extraction solvent, and heated and stirred carries out gac desorption reaction, and first quick and back slow, after desorption reaction, suction filtration goes out reaction solution to stirring velocity, and twice rinse filter cake;
(2) reaction solution underpressure distillation obtains product D IOP and solvent Virahol, and solvent recuperation is for recycle.
2. the recovery method of a kind of dioctyl phthalate (DOP) as claimed in claim 1, is characterized in that: in step (1), and the mass ratio of filter residue and alcohol is 1:(0.5 ~ 3), desorption reaction temperature is 30 ~ 100 DEG C, and the reaction times is 0.5 ~ 3 hour.
3. the recovery method of a kind of dioctyl phthalate (DOP) as claimed in claim 1 or 2, is characterized in that: in step (1), and the mass ratio of filter residue and alcohol is 1:(1 ~ 2), desorption reaction temperature is 45 ~ 70 DEG C, and the reaction times is 0.75 ~ 1.5 hour.
4. the recovery method of a kind of dioctyl phthalate (DOP) as claimed in claim 1, it is characterized in that: in step (1), stirring is divided into pre-stirring and reaction stirring, advanced line speed at the pre-stirring 5-20 minute of 80-120r/min, then carries out reaction stirring 40-60 minute under 250-400r/min speed.
5. the recovery method of a kind of dioctyl phthalate (DOP) as described in claim 1 or 3, is characterized in that: in step (1), and stir and be divided into pre-stirring and reaction stirring, pre-stirring velocity is 100r/min, and the time is 8-12 minute; Reaction stirring velocity is 300r/min, and the time is 45-55 minute.
6. the recovery method of a kind of dioctyl phthalate (DOP) as claimed in claim 1, is characterized in that: in step (1), described Extraction solvent selects the one in methyl alcohol, ethanol, propyl alcohol, Virahol, butanols, amylalcohol.
7. the recovery method of a kind of dioctyl phthalate (DOP) as claimed in claim 1, is characterized in that: in step (2), and described vacuum distillation temperature is 70 ~ 80 DEG C, and pressure is-0.1 ~-0.3MPa.
8. the recovery method of a kind of dioctyl phthalate (DOP) as described in claim 1 or 7, is characterized in that: in step (2), and vacuum distillation temperature is 78 DEG C, and pressure is-0.1 ~-0.15MPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610023975.5A CN105541628B (en) | 2016-01-14 | 2016-01-14 | A kind of recovery method of dioctyl phthalate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610023975.5A CN105541628B (en) | 2016-01-14 | 2016-01-14 | A kind of recovery method of dioctyl phthalate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105541628A true CN105541628A (en) | 2016-05-04 |
| CN105541628B CN105541628B (en) | 2017-09-29 |
Family
ID=55821247
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610023975.5A Active CN105541628B (en) | 2016-01-14 | 2016-01-14 | A kind of recovery method of dioctyl phthalate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105541628B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107281776A (en) * | 2017-07-21 | 2017-10-24 | 中国林业科学研究院林产化学工业研究所 | A kind of environmental protection treatment DOTP produces the process of waste residue recovered plasticizer |
| CN111847751A (en) * | 2020-08-29 | 2020-10-30 | 江苏美能膜材料科技有限公司 | Zero-emission recovery process for waste liquid generated by preparing polyvinylidene fluoride porous membrane |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1935776A (en) * | 2006-10-24 | 2007-03-28 | 南京大学 | Method for treating diethyl (o-) phthalate waste water and recovering diethyl (o-) phthalate from it |
| CN101530780A (en) * | 2009-04-21 | 2009-09-16 | 浙江工商大学 | Two-step separation-purification column and use thereof |
-
2016
- 2016-01-14 CN CN201610023975.5A patent/CN105541628B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1935776A (en) * | 2006-10-24 | 2007-03-28 | 南京大学 | Method for treating diethyl (o-) phthalate waste water and recovering diethyl (o-) phthalate from it |
| CN101530780A (en) * | 2009-04-21 | 2009-09-16 | 浙江工商大学 | Two-step separation-purification column and use thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107281776A (en) * | 2017-07-21 | 2017-10-24 | 中国林业科学研究院林产化学工业研究所 | A kind of environmental protection treatment DOTP produces the process of waste residue recovered plasticizer |
| CN107281776B (en) * | 2017-07-21 | 2019-07-12 | 中国林业科学研究院林产化学工业研究所 | A kind of process of environmental protection treatment DOTP production waste residue recovered plasticizer |
| CN111847751A (en) * | 2020-08-29 | 2020-10-30 | 江苏美能膜材料科技有限公司 | Zero-emission recovery process for waste liquid generated by preparing polyvinylidene fluoride porous membrane |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105541628B (en) | 2017-09-29 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106397368A (en) | Fatty alcohol-polyoxyethylene ether glycidyl ether and preparation method thereof | |
| CN111607067B (en) | Method for synthesizing epoxy resin from epichlorohydrin rectifying still residues | |
| CN107987036A (en) | A kind of propylene oxide process | |
| CN103274898A (en) | Process for recovering distillation waste liquid generated by producing 1,4-butanediol | |
| CN105541556A (en) | Neopentyl glycol and sodium formate separating method | |
| CN105541628A (en) | Method for recycling dioctyl phthalate | |
| CN105293454A (en) | Method for preparing dilute nitric acid, sponge tin and polymeric aluminum through spent tin-fading liquid | |
| CN103694101B (en) | A kind of method of comprehensive utilization of sodium hydrosulfite waste residue | |
| CN108774110B (en) | Continuous recycling process for desalting waste liquid of BDO device produced by Rebo method after steaming | |
| CN102675242A (en) | Refining method of vulkacit M | |
| CN104592160B (en) | Method for multistage washing impurity removal of rubber vulcanizing accelerator TBBS | |
| CN112999679A (en) | System and method for recovering isopropanol from waste organic solvent | |
| CN109053627A (en) | The comprehensive recovering process of 2-mercaptobenzothiazole, triethylamine and methylene chloride in Ceftriaxone Sodium methylene chloride mother liquor | |
| CN101948465A (en) | Method for preparing vitamin B1 intermediate | |
| CN107585820A (en) | A kind of extractant and extracting process to polyhydric phenols in phenol wastewater with high distribution coefficient | |
| CN107083496A (en) | A kind of method that rare earth oxide is extracted from rare earth waste | |
| CN107281776B (en) | A kind of process of environmental protection treatment DOTP production waste residue recovered plasticizer | |
| JP2018503734A (en) | Method for obtaining ore dust control resin, ore dust control resin, method for controlling ore particle emission and use of resin | |
| CN212864612U (en) | Recovery system of triethylamine for permanent violet production | |
| CN110551025B (en) | System and method for recovering and refining by-product methyl formate in coal-to-ethylene glycol process | |
| CN102659515A (en) | Method for recovering 1,4-butanediol from waste liquor generated in production of 1,4-butanediol through Reppe method | |
| CN111848353A (en) | Method for harmless recycling treatment of BDO organic waste liquid | |
| CN102451669A (en) | Method for recovering and reutilizing waste bentonite in oil refinery | |
| CN113264864A (en) | Preparation method of N, N' -m-phenylene bismaleimide | |
| CN104910142A (en) | Method for preparing vitamin B1 intermediate (pyrimidine) |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |